CN108046640B - Aliphatic superplasticizer modified by 2-naphthol waste liquid and preparation method thereof - Google Patents
Aliphatic superplasticizer modified by 2-naphthol waste liquid and preparation method thereof Download PDFInfo
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- CN108046640B CN108046640B CN201711377067.7A CN201711377067A CN108046640B CN 108046640 B CN108046640 B CN 108046640B CN 201711377067 A CN201711377067 A CN 201711377067A CN 108046640 B CN108046640 B CN 108046640B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/166—Macromolecular compounds comprising sulfonate or sulfate groups obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2/00—Addition polymers of aldehydes or cyclic oligomers thereof or of ketones; Addition copolymers thereof with less than 50 molar percent of other substances
- C08G2/30—Chemical modification by after-treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- Ceramic Engineering (AREA)
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention provides an aliphatic superplasticizer modified by 2-naphthol waste liquid and a preparation method thereof, relating to the technical field of waste liquid treatment; the traditional Chinese medicine is prepared from the following raw materials in parts by weight: 35-90 parts of 2-naphthol waste liquid, 60-80 parts of ketone compound, 380 parts of aldehyde compound 260-containing organic solvent, 80-180 parts of sodium sulfite, 5-15 parts of initiator, 3-12 parts of cellulose xanthate, 1-10 parts of sodium styrene sulfonate, 30-90 parts of calcium chloride and 160 parts of water 110-containing organic solvent; in the preparation process, firstly, mixing cellulose xanthate and sodium styrene sulfonate to prepare a solution A, then sequentially adding sodium sulfite, an initiator, a ketone compound, an aldehyde compound, the solution A and calcium chloride into the 2-naphthol waste liquid, and controlling each reaction temperature to prepare a water reducing agent; the modified water reducing agent prepared by the invention can obviously reduce slump loss, and has better slump retaining property and frost resistance compared with the common aliphatic water reducing agent.
Description
Technical Field
The invention relates to the technical field of waste liquid treatment, in particular to an aliphatic superplasticizer modified by 2-naphthol waste liquid and a preparation method thereof.
Background
The 2-naphthol is produced mainly by a naphthalene sulfonation-alkali fusion route in China and is prepared by processes of sulfonation, hydrolysis, neutralization, alkali fusion, acidification, refining and the like, in the process, waste liquid is mainly generated twice, wherein one time is mother liquid obtained after sodium naphthalenesulfonate suction filtration, and the other time is mother liquid obtained after boiling and layering crude phenol and water phase is cooled and filter-pressed.
The 2-naphthol production wastewater has the characteristics of complex components, high concentration, high toxicity, deep color, strong acid-base buffer property, difficult biochemical degradation, great harm to human bodies and environment and the like, the problem of environmental pollution caused by the above-mentioned components is not solved effectively, the treatment of the 2-naphthol waste liquid mainly adopts distillation concentration, chemical treatment and other modes, the waste liquid treatment is complex, the energy consumption is high, and the treatment cost is high.
The main components of the mother liquor after the sodium naphthalenesulfonate suction filtration comprise 2-sodium naphthalenesulfonate, sodium sulfate and the like, and the 2-sodium naphthalenesulfonate has activity and can be subjected to condensation, graft copolymerization and other reactions, so that theoretical feasibility is provided for the mother liquor participating in the modification of the aliphatic water reducer. The sodium sulfate is stable and does not participate in reactions such as sulfonation, condensation and the like, but is an early strength agent in concrete, and the sodium sulfate in the waste liquid exists in the mother liquid of the water reducing agent all the time, so that the synthesized aliphatic water reducing agent has an early strength effect.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the aliphatic high-efficiency water reducing agent modified by the waste liquid of 2-naphthol and the preparation method thereof, and the prepared water reducing agent has good early strength and antifreezing property.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a2-naphthol waste liquid modified aliphatic superplasticizer is prepared from the following raw materials in parts by weight: 35-90 parts of 2-naphthol waste liquid, 60-80 parts of ketone compound, 380 parts of aldehyde compound 260-containing material, 80-180 parts of sodium sulfite, 5-15 parts of initiator, 3-12 parts of cellulose xanthate, 1-10 parts of sodium styrene sulfonate, 30-90 parts of calcium chloride and 160 parts of water 110-containing material.
Preferably, the high-efficiency water reducing agent is prepared from the following raw materials in parts by weight: 50 parts of 2-naphthol waste liquid, 70 parts of ketone compound, 320 parts of aldehyde compound, 140 parts of sodium sulfite, 10 parts of initiator, 8 parts of cellulose xanthate, 6 parts of sodium styrene sulfonate, 55 parts of calcium chloride and 145 parts of water.
Preferably, the ketone compound is selected from one of acetone, methyl ethyl ketone and 4-methyl-2-pentanone.
Preferably, the aldehyde compound is selected from one of formaldehyde, propionaldehyde, butyraldehyde and benzaldehyde.
Preferably, the initiator is selected from one of azobisisobutyronitrile, azobisisovaleronitrile and azobiscyclohexyl carbonitrile.
A preparation method of an aliphatic superplasticizer modified by 2-naphthol waste liquid comprises the following steps: (1) mixing cellulose xanthate and sodium styrene sulfonate with water to prepare a solution A; (2) adding 2-naphthol waste liquid and sodium sulfite into water, and heating to 35-50 ℃; (3) adding an initiator and a ketone compound into the solution obtained in the step (2), raising the temperature to 50-55 ℃, and keeping the temperature for 2-3 h; continuously adding an aldehyde compound, and keeping the temperature for 1-2 h; (4) and (4) adding the solution A into the step (3), heating to 65-85 ℃, adding calcium chloride, preserving the temperature for 40-80min, and cooling to obtain the 2-naphthol waste liquid modified aliphatic superplasticizer.
(III) advantageous effects
The invention provides an aliphatic superplasticizer modified by 2-naphthol waste liquid and a preparation method thereof, wherein the aliphatic superplasticizer can be produced by directly utilizing the 2-naphthol waste liquid without any treatment, so that the wastewater discharge is reduced, the environmental pollution is avoided, the slump loss can be obviously reduced by the modified superplasticizer, and the modified superplasticizer has better slump-retaining property compared with a common aliphatic superplasticizer; the initiator can initiate the reaction of the ketone and the aldehyde compound, the cellulose xanthate can avoid the excessive crosslinking of the ketone and the aldehyde compound, and the cellulose xanthate is matched with the initiator to ensure that the reaction product reaches the optimal crosslinking degree; the sodium styrene sulfonate plays roles of flocculation and stabilization, prevents the rearrangement of the molecular structure of a reaction product, and the calcium chloride can play a role of freezing resistance, can accelerate the hardening of concrete and increase the cold resistance of the concrete.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a2-naphthol waste liquid modified aliphatic superplasticizer is prepared from the following raw materials in parts by weight: 50 parts of 2-naphthol waste liquid, 70 parts of acetone, 320 parts of formaldehyde, 140 parts of sodium sulfite, 10 parts of azobisisobutyronitrile, 8 parts of cellulose xanthate, 7 parts of sodium styrene sulfonate, 55 parts of calcium chloride and 145 parts of water. The preparation method comprises the following steps:
(1) mixing cellulose xanthate and sodium styrene sulfonate with water to prepare a solution A; (2) adding 2-naphthol waste liquid and sodium sulfite into water, and heating to 35 ℃; (3) adding azodiisobutyronitrile and acetone into the solution obtained in the step (2), raising the temperature to 52 ℃, and keeping the temperature for 3 hours; continuously adding formaldehyde, and keeping the temperature for 1 h; (4) and (4) adding the solution A into the step (3), heating to 70 ℃, adding calcium chloride, preserving the temperature for 60min, and cooling to obtain the 2-naphthol waste liquid modified aliphatic superplasticizer.
Example 2:
a2-naphthol waste liquid modified aliphatic superplasticizer is prepared from the following raw materials in parts by weight: 63 parts of 2-naphthol waste liquid, 70 parts of methyl ethyl ketone, 260 parts of propionaldehyde, 80 parts of sodium sulfite, 10 parts of azodiisovaleronitrile, 3 parts of cellulose xanthate, 5 parts of sodium styrene sulfonate, 40 parts of calcium chloride and 125 parts of water. The preparation method comprises the following steps:
(1) mixing cellulose xanthate and sodium styrene sulfonate with water to prepare a solution A; (2) adding 2-naphthol waste liquid and sodium sulfite into water, and heating to 40 ℃; (3) adding azodiisovaleronitrile and methyl ethyl ketone into the solution in the step (2), raising the temperature to 52 ℃, and keeping the temperature for 2 hours; continuously adding propionaldehyde, and keeping the temperature for 1 h; (4) and (4) adding the solution A into the step (3), heating to 70 ℃, adding calcium chloride, preserving the temperature for 50min, and cooling to obtain the 2-naphthol waste liquid modified aliphatic superplasticizer.
Example 3:
a2-naphthol waste liquid modified aliphatic superplasticizer is prepared from the following raw materials in parts by weight: 78 parts of 2-naphthol waste liquid, 75 parts of acetone, 380 parts of benzaldehyde, 130 parts of sodium sulfite, 15 parts of azodicyclohexyl formonitrile, 5 parts of cellulose xanthate, 3 parts of sodium styrene sulfonate, 75 parts of calcium chloride and 110 parts of water. The preparation method comprises the following steps:
(1) mixing cellulose xanthate and sodium styrene sulfonate with water to prepare a solution A; (2) adding 2-naphthol waste liquid and sodium sulfite into water, and heating to 45 ℃; (3) adding azodicyclohexyl formonitrile and acetone into the solution obtained in the step (2), raising the temperature to 50 ℃, and keeping the temperature for 2 hours; continuously adding benzaldehyde, and keeping the temperature for 2 hours; (4) and (4) adding the solution A into the step (3), heating to 65 ℃, adding calcium chloride, keeping the temperature for 70min, and cooling to obtain the 2-naphthol waste liquid modified aliphatic superplasticizer.
Example 4:
a2-naphthol waste liquid modified aliphatic superplasticizer is prepared from the following raw materials in parts by weight: 35 parts of 2-naphthol waste liquid, 80 parts of 4-methyl-2-pentanone, 290 parts of formaldehyde, 155 parts of sodium sulfite, 8 parts of azodiisovaleronitrile, 12 parts of cellulose xanthate, 10 parts of sodium styrene sulfonate, 90 parts of calcium chloride and 160 parts of water. The preparation method comprises the following steps:
(1) mixing cellulose xanthate and sodium styrene sulfonate with water to prepare a solution A; (2) adding 2-naphthol waste liquid and sodium sulfite into water, and heating to 50 ℃; (3) adding azodiisovaleronitrile and 4-methyl-2-pentanone into the solution obtained in the step (2), raising the temperature to 55 ℃, and preserving the temperature for 3 hours; continuously adding formaldehyde, and keeping the temperature for 2 hours; (4) and (4) adding the solution A into the step (3), heating to 85 ℃, adding calcium chloride, preserving the temperature for 80min, and cooling to obtain the 2-naphthol waste liquid modified aliphatic superplasticizer.
Example 5:
a2-naphthol waste liquid modified aliphatic superplasticizer is prepared from the following raw materials in parts by weight: 90 parts of 2-naphthol waste liquid, 60 parts of methyl ethyl ketone, 350 parts of butyraldehyde, 180 parts of sodium sulfite, 5 parts of azobisisobutyronitrile, 10 parts of cellulose xanthate, 1 part of sodium styrene sulfonate, 30 parts of calcium chloride and 110 parts of water. The preparation method comprises the following steps:
(1) mixing cellulose xanthate and sodium styrene sulfonate with water to prepare a solution A; (2) adding 2-naphthol waste liquid and sodium sulfite into water, and heating to 30 ℃; (3) adding azodiisobutyronitrile and methyl ethyl ketone into the solution obtained in the step (2), raising the temperature to 50 ℃, and keeping the temperature for 2 hours; continuously adding butyraldehyde, and keeping the temperature for 2 hours; (4) and (4) adding the solution A into the step (3), heating to 65 ℃, adding calcium chloride, preserving the temperature for 40min, and cooling to obtain the 2-naphthol waste liquid modified aliphatic superplasticizer.
The concrete performance of the modified aliphatic superplasticizer prepared in each embodiment of the invention is compared with the concrete performance of a common aliphatic superplasticizer as follows:
in summary, the embodiment of the invention has the following beneficial effects:
the invention provides a 2-naphthol waste liquid modified aliphatic high-efficiency water reducing agent and a preparation method thereof, the modified water reducing agent can obviously reduce slump loss, and has better slump retaining property and frost resistance compared with a common aliphatic water reducing agent.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (3)
1. The aliphatic superplasticizer modified by the waste liquid of 2-naphthol is characterized by being prepared from the following raw materials in parts by weight: 35-90 parts of 2-naphthol waste liquid, 60-80 parts of ketone compound, 380 parts of aldehyde compound, 80-180 parts of sodium sulfite, 5-15 parts of initiator, 3-12 parts of cellulose xanthate, 1-10 parts of sodium styrene sulfonate, 30-90 parts of calcium chloride and 160 parts of water, wherein the initiator is selected from one of azobisisobutyronitrile, azobisisovaleronitrile and azobiscyclohexylcarbonitrile; the ketone compound is selected from one of acetone, methyl ethyl ketone and 4-methyl-2-pentanone; the aldehyde compound is selected from one of formaldehyde, propionaldehyde, butyraldehyde and benzaldehyde.
2. The aliphatic superplasticizer modified by the waste liquid of 2-naphthol as claimed in claim 1, which is prepared from the following raw materials in parts by weight: 50 parts of 2-naphthol waste liquid, 70 parts of ketone compound, 320 parts of aldehyde compound, 140 parts of sodium sulfite, 10 parts of initiator, 8 parts of cellulose xanthate, 6 parts of sodium styrene sulfonate, 55 parts of calcium chloride and 145 parts of water.
3. The preparation method of the aliphatic superplasticizer modified by the waste liquid of 2-naphthol according to any one of claims 1 to 2, characterized by comprising the following steps: (1) mixing cellulose xanthate and sodium styrene sulfonate with water to prepare a solution A; (2) adding 2-naphthol waste liquid and sodium sulfite into water, and heating to 35-50 ℃; (3) adding an initiator and a ketone compound into the solution obtained in the step (2), raising the temperature to 50-55 ℃, and keeping the temperature for 2-3 h; continuously adding an aldehyde compound, and keeping the temperature for 1-2 h; (4) and (4) adding the solution A into the step (3), heating to 65-85 ℃, adding calcium chloride, preserving the temperature for 40-80min, and cooling to obtain the 2-naphthol waste liquid modified aliphatic superplasticizer.
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CN102875049A (en) * | 2012-11-01 | 2013-01-16 | 徐友娟 | High sulfonation degree aliphatic water reducing agent and preparation method thereof |
CN103641354A (en) * | 2013-11-29 | 2014-03-19 | 山东七星岩建材科技有限公司 | Environment-friendly concrete superplasticizer and preparation method thereof |
CN104860568A (en) * | 2015-04-21 | 2015-08-26 | 萧县沃德化工科技有限公司 | Highly-efficient aliphatic water reducer modified by 2-naphthol waste liquor and preparation method thereof |
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EP1024120B1 (en) * | 1999-01-29 | 2012-03-07 | Sika Technology AG | Method of reducing the shrinkage of hydraulic binders |
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CN102875049A (en) * | 2012-11-01 | 2013-01-16 | 徐友娟 | High sulfonation degree aliphatic water reducing agent and preparation method thereof |
CN103641354A (en) * | 2013-11-29 | 2014-03-19 | 山东七星岩建材科技有限公司 | Environment-friendly concrete superplasticizer and preparation method thereof |
CN104860568A (en) * | 2015-04-21 | 2015-08-26 | 萧县沃德化工科技有限公司 | Highly-efficient aliphatic water reducer modified by 2-naphthol waste liquor and preparation method thereof |
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